EP0554896A1 - Articles composites comprenant une étoffe non-tissée et un film de polyoléfine, et procédé de leur fabrication - Google Patents

Articles composites comprenant une étoffe non-tissée et un film de polyoléfine, et procédé de leur fabrication Download PDF

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Publication number
EP0554896A1
EP0554896A1 EP19930101832 EP93101832A EP0554896A1 EP 0554896 A1 EP0554896 A1 EP 0554896A1 EP 19930101832 EP19930101832 EP 19930101832 EP 93101832 A EP93101832 A EP 93101832A EP 0554896 A1 EP0554896 A1 EP 0554896A1
Authority
EP
European Patent Office
Prior art keywords
propylene
ethylene
film
copolymer
article
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
EP19930101832
Other languages
German (de)
English (en)
Other versions
EP0554896B1 (fr
Inventor
Guiseppe Lesca
Vincenzo Gianella
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Moplefan SpA
Basell North America Inc
Original Assignee
Moplefan SpA
Himont Inc
Montell North America Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Moplefan SpA, Himont Inc, Montell North America Inc filed Critical Moplefan SpA
Publication of EP0554896A1 publication Critical patent/EP0554896A1/fr
Application granted granted Critical
Publication of EP0554896B1 publication Critical patent/EP0554896B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
    • B32B5/022—Non-woven fabric
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
    • C08F297/06—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type
    • C08F297/08—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins
    • C08F297/083—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins the monomers being ethylene or propylene
    • C08F297/086—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins the monomers being ethylene or propylene the block polymer contains at least three blocks
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0253—Polyolefin fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/31—Heat sealable
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/08—Dimensions, e.g. volume
    • B32B2309/10—Dimensions, e.g. volume linear, e.g. length, distance, width
    • B32B2309/105—Thickness
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/31504—Composite [nonstructural laminate]
    • Y10T428/31855—Of addition polymer from unsaturated monomers
    • Y10T428/31909—Next to second addition polymer from unsaturated monomers
    • Y10T428/31913—Monoolefin polymer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T442/00—Fabric [woven, knitted, or nonwoven textile or cloth, etc.]
    • Y10T442/60—Nonwoven fabric [i.e., nonwoven strand or fiber material]
    • Y10T442/674—Nonwoven fabric with a preformed polymeric film or sheet
    • Y10T442/678—Olefin polymer or copolymer sheet or film [e.g., polypropylene, polyethylene, ethylene-butylene copolymer, etc.]

Definitions

  • the present invention concerns articles comprising a polypropylene nonwoven fabric (NWF) bonded with a polyolefin film, and the process for their preparation.
  • NWF polypropylene nonwoven fabric
  • Articles consisting of a thin nonwoven fabric bonded with polyolefin film are well known and commercially available and are found in a number of applications, for example coverstock for sanitary napkins, gowns and protective clothing for the medical sector, disposable tablecloths and sheets.
  • the material which forms the thin NWF is obtained from polypropylene fibers, cohered by passing them through a carding machine ("card web"), or thermosealed by way of calendering.
  • the films used for the production of the above mentioned articles consist of homo- and copolymers of ethylene, particularly low density polyethylene (LDPE), linear low density polyethylene (LLDPE), ethylene/vinyl acetate copolymers (EVA), high density polyethylene (HDPE), or a mixture of two or more of said polymers.
  • LDPE low density polyethylene
  • LLDPE linear low density polyethylene
  • EVA ethylene/vinyl acetate copolymers
  • HDPE high density polyethylene
  • thermobonding optionally using the thermosealing by points method.
  • This type of sealing is very difficult because of the different chemical nature of the two layers. Only by using high temperatures and long periods of time could one partially achieve said bonding (with poor results), by causing the partially melted film to penetrate the NWF; however, the article obtained with this method would be even more rigid and paper-like than the one produced by using the adhesives.
  • the articles of the present invention comprise a polypropylene nonwoven fabric bonded directly to a film made of a heterophasic polymer composition comprising (percentage by weight):
  • copolymer (C) of the heterophasic polymer composition comprises a diene
  • the latter is present preferably in quantities lower than or equal to 10% by weight.
  • preferred dienes are: 1,4-hexadiene; dicyclopentadiene; and 2-ethylidene-5-norbornene.
  • Examples of preferred ⁇ -olefins having 4-10 carbon atoms that can be present in (A) and in (C) are: 1-butene, 4-methyl-1-pentene and 1-hexene.
  • the polypropylene fiber used for the preparation of the nonwoven fabric can be any of the commercially available heat sealable fibers, generally comprising crystalline polymers, in particular homopolymers having melt index values (230 o C, 2.16 Kg, ASTM D1238 method, condition L) of 10-30 g/10 min and an isotactic index of ⁇ 85.
  • heterophasic polymer compositions used for the films used in the articles of the present invention are preferably prepared by way of sequential polymerization in two or more stages, using highly stereospecific Ziegler-Natta catalysts.
  • Component (A) is formed in the first stages of polymerization, preferably in liquid monomer, while (B) and (C) are formed in one or more subsequent polymerization stages.
  • the catalysts that can be used in particular are those comprising the reaction product of a solid component containing a titanium compound and an electron-donor compound (internal donor) supported on activated magnesium chloride, with an Altrialkyl compound and an electron-donor compound (external donor).
  • the titanium compound used is the TiCl4.
  • the internal donor is preferably selected from the alkyl, cycloalkyl or aryl phthalates, such as for example diisobutyl, di-n-butyl and di-n-octyl phthalate.
  • the external donor is selected preferably from the silicon compounds containing one or more -OR groups, where R is a hydrocarbon radical.
  • R is a hydrocarbon radical.
  • Specific examples are diphenyldimethoxysilane, dicyclohexyldimethoxysilane, methyl-tert-butyldimethoxysilane diisopropyldimethoxysilane and phenyltriethoxysilane.
  • the heterophasic composition of the invention can also be obtained by mechanical blending of component (A), which is prepared separately, and products (B) and (C).
  • the product of (B) + (C) can be obtained by copolymerizing ethylene with propylene and/or an ⁇ -olefin having 4-10 carbon atoms, and optionally a diene, in the presence of a catalyst of the types described above.
  • Processes suitable for use in producing the film of the above heterophasic compositions are those known in the art and are, for example, blow-molding, cast-extrusion and bioriented-extrusion.
  • the thickness of the films is preferably from 10 to 50 ⁇ m. Examples of films obtained from heterophasic compositions of the type described above are given in published European patent application n. 444 671.
  • the polypropylene film and the NWF are heat sealed operating at a temperature preferably ranging from 90 to 140 o C. Because of the particular physico-chemical nature of the film material, these temperature conditions are sufficient to cause the bonding of the two layers, and provide a product with good flexibility, noiselessness, softness, pleasing touch, and freedom from solvents and/or adhesive substances.
  • the heat-seal operation is carried out according to known techniques, overlapping the two layers, and using a calender, or another device which allows the effective compression of one layer against the other at an appropriate temperature.
  • a calender which comprises one smooth roller and one embossed roller
  • a nonwoven fabric with an average denier equal to 20 g/m3
  • the film and the nonwoven fabric described above are then subjected to bonding using the same calender that was used to produce the nonwoven fabric, to which has been added a film-feeding device.
  • the film and the nonwoven fabric are fed respectively in contact with the smooth roller and the embossed roller.
  • the speed with which the film and the NWF are fed is maintained constant, throughout the test, at 70 m/min; the temperature of the smooth roller is 105 o C, while that of the embossed roller is 125 o C.
  • the bonding of the two layers is excellent, and the article obtained, with a denier of about 30 g/m2, is very flexible, soft and noiseless.
  • Example 1 is repeated by bonding the same nonwoven with a 15 micrometers thick film made of LDPE having a melt index (190 o C 2.16 Kg, ASTM D 1238, condition E) equal to 6 g/10 min, and density of 0.92 g/cm3, prepared by blow-molding.
  • a melt index 190 o C 2.16 Kg, ASTM D 1238, condition E
  • density 0.92 g/cm3, prepared by blow-molding.
EP19930101832 1992-02-06 1993-02-05 Articles composites comprenant une étoffe non-tissée et un film de polyoléfine, et procédé de leur fabrication Expired - Lifetime EP0554896B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
ITMI920233 1992-02-06
IT92MI233 IT1254202B (it) 1992-02-06 1992-02-06 Manufatti accoppiati comprendenti un tessuto-non-tessuto e un film in materiali poliolefinici e procedimento per la loro preparazione

Publications (2)

Publication Number Publication Date
EP0554896A1 true EP0554896A1 (fr) 1993-08-11
EP0554896B1 EP0554896B1 (fr) 1998-11-18

Family

ID=11361831

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19930101832 Expired - Lifetime EP0554896B1 (fr) 1992-02-06 1993-02-05 Articles composites comprenant une étoffe non-tissée et un film de polyoléfine, et procédé de leur fabrication

Country Status (10)

Country Link
US (1) US5368927A (fr)
EP (1) EP0554896B1 (fr)
AT (1) ATE173432T1 (fr)
CA (1) CA2088708C (fr)
CZ (1) CZ282571B6 (fr)
DE (1) DE69322107T2 (fr)
ES (1) ES2125916T3 (fr)
IL (1) IL104488A0 (fr)
IT (1) IT1254202B (fr)
TW (1) TW213497B (fr)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994009193A1 (fr) * 1992-10-09 1994-04-28 Moplefan S.P.A. Composition polymere pour des fibres de polypropylene souples
WO1996034741A1 (fr) * 1995-05-02 1996-11-07 Kimberly-Clark Worldwide, Inc. Stratifies a films et a non-tisses
US5763041A (en) * 1995-12-21 1998-06-09 Kimberly-Clark Worldwide, Inc. Laminate material
US5910136A (en) * 1996-12-30 1999-06-08 Kimberly-Clark Worldwide, Inc. Oriented polymeric microporous films with flexible polyolefins
US5914184A (en) * 1996-12-30 1999-06-22 Kimberly-Clark Worldwide, Inc. Breathable laminate including filled film and continuous film
WO1999040160A1 (fr) * 1998-02-03 1999-08-12 Montell Technology Company B.V. Composition adhesive thermofusible a base de polyolefines
US5947944A (en) * 1996-12-30 1999-09-07 Kimberly-Clark Worldwide, Inc. Stretched-thinned films comprising low crystallinity polymers and laminates thereof
FR2803606A1 (fr) * 2000-01-12 2001-07-13 Pennel Ind Sa Textile enduit imprime a base d'un composant polyolefinique

Families Citing this family (25)

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Publication number Priority date Publication date Assignee Title
US5482772A (en) * 1992-12-28 1996-01-09 Kimberly-Clark Corporation Polymeric strands including a propylene polymer composition and nonwoven fabric and articles made therewith
US5460884A (en) * 1994-08-25 1995-10-24 Kimberly-Clark Corporation Soft and strong thermoplastic polymer fibers and nonwoven fabric made therefrom
US5814178A (en) * 1995-06-30 1998-09-29 Kimberly-Clark Worldwide, Inc. Process for making a bulked fabric laminate
US5662978A (en) * 1995-09-01 1997-09-02 Kimberly-Clark Worldwide, Inc. Protective cover fabric including nonwovens
US5795834A (en) * 1995-12-22 1998-08-18 Minnesota Mining & Manufacturing Company Adhesive tape and method of making
US6103647A (en) * 1996-03-14 2000-08-15 Kimberly-Clark Worldwide, Inc. Nonwoven fabric laminate with good conformability
US6037281A (en) 1996-12-27 2000-03-14 Kimberly-Clark Worldwide, Inc. Cloth-like, liquid-impervious, breathable composite barrier fabric
US5964743A (en) * 1997-02-27 1999-10-12 Kimberly-Clark Worldwide, Inc. Elastic absorbent material for personal care products
US6080818A (en) * 1997-03-24 2000-06-27 Huntsman Polymers Corporation Polyolefin blends used for non-woven applications
US6589638B1 (en) * 1997-09-15 2003-07-08 Kimberly-Clark Worldwide, Inc. Stretch-pillowed bulked laminate useful as an ideal loop fastener component
US6610163B1 (en) 1997-12-17 2003-08-26 Kimberly-Clark Worldwide, Inc. Enhanced barrier film and laminate and method for producing same
US6013151A (en) * 1998-05-15 2000-01-11 Clopay Plastic Products Company, Inc. High speed method of making microporous film products
US6265045B1 (en) * 1998-07-29 2001-07-24 Clopay Plastic Products Company, Inc. Method and apparatus for pin-hole prevention in zone laminates
US6649548B1 (en) 1998-10-02 2003-11-18 Kimberly-Clark Worldwide, Inc. Nonwoven web and film laminate with improved strength and method of making the same
US6682803B2 (en) 1999-08-27 2004-01-27 Kimberly-Clark Worldwide, Inc. Breathable multilayer films with breakable skin layers
US20030203231A1 (en) * 2002-04-30 2003-10-30 Kimberly-Clark Worldwide, Inc. UV stabilization of synthetic paper
CN101006152B (zh) * 2004-06-28 2012-02-08 陶氏环球技术有限责任公司 用于多结构层压材料的增粘剂
US20060251858A1 (en) * 2005-05-06 2006-11-09 Kimberly-Clark Worldwide, Inc. Elastic, breathable barrier films and laminates
US9168720B2 (en) 2009-02-27 2015-10-27 Exxonmobil Chemical Patents Inc. Biaxially elastic nonwoven laminates having inelastic zones
US9168718B2 (en) 2009-04-21 2015-10-27 Exxonmobil Chemical Patents Inc. Method for producing temperature resistant nonwovens
US8664129B2 (en) 2008-11-14 2014-03-04 Exxonmobil Chemical Patents Inc. Extensible nonwoven facing layer for elastic multilayer fabrics
US9498932B2 (en) 2008-09-30 2016-11-22 Exxonmobil Chemical Patents Inc. Multi-layered meltblown composite and methods for making same
US10161063B2 (en) 2008-09-30 2018-12-25 Exxonmobil Chemical Patents Inc. Polyolefin-based elastic meltblown fabrics
US8668975B2 (en) 2009-11-24 2014-03-11 Exxonmobil Chemical Patents Inc. Fabric with discrete elastic and plastic regions and method for making same
KR101307987B1 (ko) * 2012-12-13 2013-09-12 서범수 자유로운 겉감 선택이 가능한 다운쟈켓

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US4748070A (en) * 1986-03-24 1988-05-31 Hercules Incorporated Film/fiber laminates
EP0444671A2 (fr) * 1990-02-28 1991-09-04 Montell North America Inc. ProcédÀ© de préparation de films de polypropylène et laminés et produits obtenus à partir de ceux-ci
EP0477662A2 (fr) * 1990-09-28 1992-04-01 Himont Incorporated Films de polymères d'oléfines

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994009193A1 (fr) * 1992-10-09 1994-04-28 Moplefan S.P.A. Composition polymere pour des fibres de polypropylene souples
WO1996034741A1 (fr) * 1995-05-02 1996-11-07 Kimberly-Clark Worldwide, Inc. Stratifies a films et a non-tisses
US5900306A (en) * 1995-05-02 1999-05-04 Kimberly-Clark Worldwide, Inc. Nonwoven-film laminates
KR100417354B1 (ko) * 1995-05-02 2004-04-21 킴벌리-클라크 월드와이드, 인크. 부직포-필름적층체
CN1077030C (zh) * 1995-05-02 2002-01-02 金伯利-克拉克环球有限公司 非织造织物－薄膜层合制品
US6190758B1 (en) 1995-05-02 2001-02-20 Kimberly-Clark Worldwide, Inc. Nonwoven-film laminates
US5763041A (en) * 1995-12-21 1998-06-09 Kimberly-Clark Worldwide, Inc. Laminate material
US5993589A (en) * 1996-12-30 1999-11-30 Morman; Michael T. Breathable laminate including filled film and continuous film and method for making the same
US5947944A (en) * 1996-12-30 1999-09-07 Kimberly-Clark Worldwide, Inc. Stretched-thinned films comprising low crystallinity polymers and laminates thereof
US6002064A (en) * 1996-12-30 1999-12-14 Kimberly-Clark Worldwide, Inc. Stretch-thinned breathable films resistant to blood and virus penetration
US5914184A (en) * 1996-12-30 1999-06-22 Kimberly-Clark Worldwide, Inc. Breathable laminate including filled film and continuous film
US5910136A (en) * 1996-12-30 1999-06-08 Kimberly-Clark Worldwide, Inc. Oriented polymeric microporous films with flexible polyolefins
WO1999040160A1 (fr) * 1998-02-03 1999-08-12 Montell Technology Company B.V. Composition adhesive thermofusible a base de polyolefines
US6486246B1 (en) 1998-02-03 2002-11-26 Montell Technology Company Bv Polyolefin based hot melt adhesive composition
FR2803606A1 (fr) * 2000-01-12 2001-07-13 Pennel Ind Sa Textile enduit imprime a base d'un composant polyolefinique
EP1116814A1 (fr) * 2000-01-12 2001-07-18 Pennel Industries S.A. Textile enduit imprimé à base d'un composant polyoléfinique

Also Published As

Publication number Publication date
ITMI920233A0 (it) 1992-02-06
ES2125916T3 (es) 1999-03-16
CA2088708A1 (fr) 1993-08-07
DE69322107T2 (de) 1999-05-20
TW213497B (fr) 1993-09-21
CZ14593A3 (en) 1993-11-17
DE69322107D1 (de) 1998-12-24
CZ282571B6 (cs) 1997-08-13
EP0554896B1 (fr) 1998-11-18
CA2088708C (fr) 1999-08-03
ITMI920233A1 (it) 1993-08-06
US5368927A (en) 1994-11-29
ATE173432T1 (de) 1998-12-15
IT1254202B (it) 1995-09-14
IL104488A0 (en) 1993-05-13

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